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WO2009067652A2 - Détection et quantification d'indicateur in situ pour corrélation avec un additif - Google Patents

Détection et quantification d'indicateur in situ pour corrélation avec un additif Download PDF

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Publication number
WO2009067652A2
WO2009067652A2 PCT/US2008/084320 US2008084320W WO2009067652A2 WO 2009067652 A2 WO2009067652 A2 WO 2009067652A2 US 2008084320 W US2008084320 W US 2008084320W WO 2009067652 A2 WO2009067652 A2 WO 2009067652A2
Authority
WO
WIPO (PCT)
Prior art keywords
additive
concentration
tracer
article
carrier material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/US2008/084320
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English (en)
Other versions
WO2009067652A3 (fr
Inventor
Ivan Wei-Kang Ong
Franklin Wrenn Wilkinson
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Microban Products Co
Original Assignee
Microban Products Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Microban Products Co filed Critical Microban Products Co
Priority to EP08851174.6A priority Critical patent/EP2223102A4/fr
Priority to AU2008326340A priority patent/AU2008326340A1/en
Publication of WO2009067652A2 publication Critical patent/WO2009067652A2/fr
Publication of WO2009067652A3 publication Critical patent/WO2009067652A3/fr
Anticipated expiration legal-status Critical
Priority to AU2015200925A priority patent/AU2015200925B2/en
Ceased legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
    • G01T1/36—Measuring spectral distribution of X-rays or of nuclear radiation spectrometry
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/07—Investigating materials by wave or particle radiation secondary emission
    • G01N2223/076—X-ray fluorescence
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/30—Accessories, mechanical or electrical features
    • G01N2223/301—Accessories, mechanical or electrical features portable apparatus
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/60—Specific applications or type of materials
    • G01N2223/623—Specific applications or type of materials plastics

Definitions

  • the present invention relates to the qualitative and/or quantitative measurement of a manufacturing additive, and in particular to a compound and method for detecting a compound and quantitatively measuring same to correlate with an added amount of one or more antimicrobial agents.
  • FIG. 1 is a flowchart diagram showing steps in an X-ray fluorescence detection scheme.
  • FIG. 2 is a diagram of a handheld X-ray fluorescence analyzer in use on a sample as described herein.
  • antimicrobial as used herein includes biostatic activity, i.e., where the proliferation of microbiological species is reduced or eliminated, and true biocidal activity where microbiological species are killed.
  • microbe or “antimicrobial” should be interpreted to specifically encompass bacteria and fungi as well as other single-celled organisms such as mold, mildew and algae.
  • a “material” may be a chemical element, a compound or mixture of chemical elements, or a compound or mixture of a compound or mixture of chemical elements, wherein the complexity of a compound or mixture may range from being simple to complex.
  • Electrodes means a chemical element of the periodic table of elements, including elements that may be discovered after the filing date of this application.
  • an antimicrobial article a quantity of an antimicrobial agent is compounded with the base resin from which the article is to be made, resulting in a masterbatch having the antimicrobial agent incorporated therein at a higher concentration than the final target concentration in the finished polymer article.
  • the masterbatch resin is mixed with unadulterated resin (e.g., in pellet form) in a specific ratio conventionally known as a letdown rate. In this manner, the additive components of the masterbatch resin are diluted into the polymer resin mixture to achieve the desired final concentration.
  • Examples of polymer goods include, without limitation, cutting boards, food and household storage containers, trash cans, footwear outsoles, caulking, filtration elements for water and air filters, Jacuzzi and whirlpool spas and tubs, computer peripheral devices, and automobile components and aftermarket parts.
  • concentrations of antimicrobial agents in polymer articles are as low as about 50 ppm, based upon the weight of the cementitious composition.
  • a practical upper end to the useful concentration range is dependent on the antimicrobial agent, the material in which it is incorporated, and the intended use environment of the article.
  • antimicrobial agent concentrations may range as high as about 100,000 ppm.
  • additives similarly can be used in the production of the material.
  • additives include, without limitation, pigments and colorants, binders, plasticizers, anti-fouling or antimicrobial agents, anti-static agents, flame retardants, processing aids (e.g. antislip agents, lubricants), heat stabilizers, ultraviolet radiation stabilizers, ultraviolet radiation absorbers, and the like
  • processing aids e.g. antislip agents, lubricants
  • heat stabilizers e.g. antislip agents, lubricants
  • ultraviolet radiation stabilizers e.g. antislip agents, lubricants
  • a product in a second embodiment, can be a cementitious article such as a grout mixture, a cement-based tile, a sculpture or decorative item, a countertop material, a building or construction article, and the like.
  • an antimicrobial agent or other additive can be introduced directly into the cement-based mixture in dry form (e.g., powder) or liquid stream.
  • the additive can be compounded with other components of the cementitious composition from which the article will be made.
  • the concentration of the antimicrobial agent can be in a range from about 250 ppm to about 10,000 ppm based upon the weight of the cementitious composition.
  • the manufactured article can be a textile good or a textile-based good.
  • An example of such goods include, without limitation, goods manufactured in whole or in part with synthetic fibers having an antimicrobial agent incorporated therein.
  • the concentration of the antimicrobial agent can be in a range from about 250 ppm to about 10,000 ppm.
  • the specific concentration would be selected in large part based on the polymer, the antimicrobial agent(s) employed, the polymer manufacturing method, any post-polymerization treatments and/or finishing steps applied to the textile, and the like.
  • X-ray fluorescence spectroscopy has long been a useful analytical tool in the laboratory for classifying materials by identifying elements within the material, both in academic environments and in industry.
  • characteristic x-rays such as, for example, K-shell or L-shell x-rays, emitted under excitation provides a method for positive identification of elements and their relative amounts present in different materials, such as metals and metal alloys.
  • input radiation striking matter causes the emission of characteristic K-shell x-rays when a K-shell electron is knocked out of the K-shell by incoming radiation and is then replaced by an outer shell electron.
  • the outer electron in dropping to the K-shell energy state, emits x-ray radiation characteristics of the atom.
  • the energy of emitted x-rays depends on the atomic number of the fluorescing elements. Energy-resolving detectors can detect the different energy levels at which x-rays are fluoresced, and generate an x- ray signal from the detected x-rays.
  • This x-ray signal may then be used to build an energy spectrum of the detected x-rays, and from the information, the element or elements which produced the x-rays may be identified.
  • Output fluorescent x-rays are emitted isotopically from an irradiated element 10, and the detected output radiation depends on the solid angle subtended by the detector 12 and any absorption of this radiation prior to the radiation reaching the detector (FIG. 1 ).
  • raw detection data is outputted from the detector 12 to electronics 14, which can assess the incoming raw data (e.g. wavelength and pattern matching, as discussed above).
  • electronics 14 can assess the incoming raw data (e.g. wavelength and pattern matching, as discussed above).
  • computer 16 can be employed to analyze and/or display detection results.
  • the amount of x-rays detected is a function of the quantity of x-rays emitted, the energy level of the emitted x-rays, the emitted x-rays absorbed in the transmission medium, the angles between the detected x-rays and the detector, and the distance between the detector and the irradiated material.
  • the unit can be employed to detect a broad variety of indicators, including without limitation titanium, chromium, manganese, iron, nickel, copper, zinc, arsenic, rubidium, strontium, zirconium, cadmium, tin, antimony, barium, mercury, lead, silver, selenium, cobalt, tungsten, bromine, and thallium.
  • an indicator can be a compound comprising one or more of the above elements.
  • the specific identity of the antimicrobial agent(s) used is not critical to the present indicator technology. It is significant only that an additive compound be added, and that a need exists to conveniently assess the article to determine if the additive has been incorporated into it and, optionally, at what level.
  • the use of XRF technology is employed advantageously to detect the presence of one or more indicators (i.e., tracer elements) in the manufactured good.
  • a first indicator can be compounded into a polymeric masterbatch at a predetermined concentration.
  • the additive e.g. antimicrobial agent
  • the ratio of additive to indicator is constant and known to the user.
  • (target) additive concentration in the finished article is known. It is therefore anticipated by the user that the antimicrobial agent additive: (a) be present in the polymer material of the manufactured article, and (b) at a predetermined final concentration. The indicator likewise is expected to be present in the finished article at a predetermined concentration.
  • an initial concern arises as to whether or not the additive, by way of masterbatch, is correctly introduced into the manufacturing process. As a first matter, then, the manufacturing process can be quantitatively assessed to verify that the masterbatch was successfully added to the polymer starting material. Quantitative analysis using the present indicator composition and methodology can be understood by review of the following example.
  • EVA masterbatch An ethyl vinyl chloride (EVA) masterbatch was prepared incorporating Additive ZO1 TM (Microban Products Company, Huntersville, North Carolina), such that the masterbatch contained the antimicrobial agent zinc pyrithione at a concentration of 100,000 ppm by weight of the EVA masterbatch.
  • Additive ZO1 TM Microban Products Company, Huntersville, North Carolina
  • Zirconium dioxide was used as an indicator at 6477.5 ppm by weight of the EVA masterbatch.
  • Zirconium was chosen as the indicator because it is unique, inert with respect to the polymer material, not present in unadulterated EVA polymer compositions, and easy to quantitatively analyze.
  • the user Rather than analyzing for zinc pyrithione directly, the user instead analyzes for the zirconium tracer, which tells how much zinc pyrithione is present in the EVA sample material. [0049]
  • the inventive masterbatch was used at a letdown ratio of
  • the theoretical concentrations of zinc pyrithione and zirconium dioxide in the exemplary manufactured article are 1500 ppm and 97.16 ppm, respectively.
  • Many other ingredients can mask the presence of the zinc pyrithione, making it difficult to conventionally analyze the treated material for this compound's presence and concentration. It is desirable to easily determine if the article manufacturer has correctly added zinc pyrithione to ensure product performance conferred by antimicrobial agent addition.
  • XRF measurements were made with an Alpha 4000
  • Handheld X-Ray Fluorescence Analyzer (Innov-X Systems, Woburn, Massachusetts) driven by an HP iPAQ PocketPC device (Hewlett- Packard, Palo Alto, California).
  • Use of the Alpha 4000 analyzer is straightforward: the user holds the nose of the Alpha 4000 analyzer (D in FGI. 2) against the sample material and pulls the trigger (FIG. 2). The instrument reads for approximately 20-30 seconds — with longer readings resulting in greater accuracy — and displays the concentration readings.
  • a palm-top computing device is built into the XRF instrument and provides both analysis and a user interface.
  • the Alpha 4000 analyzer can be used to measure for any of several different indicators.
  • the Alpha 4000 analyzer and methodology as described above can further be employed to determine the concentration of indicator in the EVA outsole article.
  • the outsole material was analyzed at three stages in manufacture: thin sheet (2 mm thick), slit foam (4 mm), and thick foam (36 mm), for each stage, three pieces were used, with each piece assayed at two different locations.
  • zirconium was detected in samples. The mean levels of zirconium observed in the three stages were 164 ppm, 205 ppm, and 148 ppm, respectively. Based on the concentration of zirconium in the masterbatch (6477.5 ppm), an actual letdown rate of -2.66% initially was calculated. This information can be useful in guiding adjustments to the manufacturing process in order to achieve the target result in the finished good.
  • the concentration of additive (e.g. antimicrobial agent) in the finished article can be calculated by reference to either the observed concentration of indicator in the article or a lookup table of output radiation signal strengths and additive concentrations.
  • concentration of additive e.g. antimicrobial agent
  • concentration of additive in the finished article can be calculated by reference to either the observed concentration of indicator in the article or a lookup table of output radiation signal strengths and additive concentrations.
  • the ratio of zinc pyrithione to zirconium dioxide in the masterbatch was 15.438:1. Using this ratio, it was calculated that the zinc level in the three stage samples was 2532 ppm, 3165 ppm, and 2285 ppm, respectively.
  • XRF analysis was undertaken directly for zinc.
  • Zinc pyrithione is useful for this example, as zinc can itself be assayed in the finished good using XRF technology. This compound therefore permitted direct-measurement confirmation of the zinc pyrithione concentration calculated using the zirconium correlation data.
  • the present method can be employed with a variety of non-metallic antimicrobial agents, as well as other additives as previously mentioned. Qualitative analysis is rapid and sufficiently accurate to be useful in manufacturing; after proper calibration, the present method can be advantageously employed to assess and/or optimize letdown rates.
  • Energy dispersive X-ray spectroscopy is a similar detection technology which can be employed in place of or in addition to X-ray fluorescence.
  • An EDX system generally is sized to sit on a bench or counter top and frequently is used in tandem with scanning electron microscopy.
  • a detector is used to convert X-ray energy into voltage signals; this information is sent to a pulse processor, which must measure the signals and pass them onto an analyzer for data display and analysis.
  • an electron or photon beam is aimed into the sample to be characterized.
  • an atom within the sample contains ground state (unexcited) electrons situated in concentric shells around the nucleus.
  • the incident beam excites an electron in an inner shell, prompting its ejection and resulting in the formation of an electron hole within the atom's electronic structure.
  • An electron from an outer, higher-energy shell then fills the hole, and the excess energy of that electron is released in the form of an X-ray.
  • the release of X-rays creates spectral lines that are highly specific to individual elements; thus, the X-ray emission data can be analyzed to characterize the sample in question.
  • Information on the quantity and kinetic energy of ejected electrons is used to determine the binding energy of the liberated electrons. Binding energy is element-specific and thus allows chemical characterization of a test sample.
  • the present method compares the plurality of indicators and applies the known ratio from the masterbatch to determine letdown rate and/or concentration.
  • a mixture of strontium and rubidium is particularly advantageous for most polymer compositions. These elements are unlikely to be found in the base resin or in chemicals used in manufacturing, such as catalysts.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • General Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Molecular Biology (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

L'invention concerne une formulation d'additif comprenant un matériau vecteur, un premier additif présent dans le matériau vecteur à une première concentration en additif, et un traceur présent dans le matériau vecteur à une première concentration en traceur. Le traceur est un métal prédisposé à une détection par analyse de fluorescence aux rayons X. Des modes de réalisation supplémentaires comprennent un article manufacturé incorporant la formulation d'additif. Un procédé est également révélé pour détecter un additif dans un article manufacturé, le procédé impliquant l'application d'une analyse de fluorescence aux rayons X de l'élément traceur.
PCT/US2008/084320 2007-11-21 2008-11-21 Détection et quantification d'indicateur in situ pour corrélation avec un additif Ceased WO2009067652A2 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
EP08851174.6A EP2223102A4 (fr) 2007-11-21 2008-11-21 Détection et quantification d'indicateur in situ pour corrélation avec un additif
AU2008326340A AU2008326340A1 (en) 2007-11-21 2008-11-21 In situ indicator detection and quantitation to correlate with an additive
AU2015200925A AU2015200925B2 (en) 2007-11-21 2015-02-24 In Situ Indicator Detection and Quantitation to Correlate with an Additive

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US98973707P 2007-11-21 2007-11-21
US60/989,737 2007-11-21

Publications (2)

Publication Number Publication Date
WO2009067652A2 true WO2009067652A2 (fr) 2009-05-28
WO2009067652A3 WO2009067652A3 (fr) 2009-08-06

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Family Applications (1)

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PCT/US2008/084320 Ceased WO2009067652A2 (fr) 2007-11-21 2008-11-21 Détection et quantification d'indicateur in situ pour corrélation avec un additif

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US (1) US20090129541A1 (fr)
EP (1) EP2223102A4 (fr)
AU (2) AU2008326340A1 (fr)
WO (1) WO2009067652A2 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110243810A (zh) * 2019-07-01 2019-09-17 中国第一汽车股份有限公司 一种金属材料表面转化膜中锆含量的测试方法
CN110261198A (zh) * 2019-07-01 2019-09-20 中国第一汽车股份有限公司 一种金属材料表面转化膜中含锆标准测试板的制备方法及其定量方法

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ITMO20100165A1 (it) * 2010-06-08 2011-12-09 Eugenio Cavallini Metodo anticontraffazione applicato a prodotti di materia plastica e plastica inglobante un codice di autenticazione anticontraffazione.
SG194862A1 (en) 2011-05-24 2013-12-30 Agienic Inc Compositions and methods for antimicrobial metal nanoparticles
US9155310B2 (en) 2011-05-24 2015-10-13 Agienic, Inc. Antimicrobial compositions for use in products for petroleum extraction, personal care, wound care and other applications
DE102015221323B3 (de) * 2015-10-30 2016-08-04 Airbus Defence and Space GmbH Verfahren zum Nachweis von Oberflächenverunreinigungen mittels Röntgenfluoreszenzanalyse
JP7062648B2 (ja) * 2016-10-10 2022-05-06 セキュリティ マターズ リミテッド Ｘｒｆ特定可能透明ポリマー
AU2020210650B2 (en) 2019-01-25 2021-03-18 Allied Bioscience, Inc. Analysis of antimicrobial coatings using XRF
KR20220035427A (ko) * 2019-07-15 2022-03-22 시큐리티 매터스 엘티디. 생산 가치 체인의 투명성을 제공하기 위한 추적 가능한 복합체 중합체 및 이의 제조 방법

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US20030133537A1 (en) 2001-12-05 2003-07-17 Fred Schramm Methods for identification and verification using vacuum XRF system

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GB1017595A (en) * 1962-06-20 1966-01-19 Atomic Energy Authority Uk Improvements in or relating to radiometric analysis techniques
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WO2002068945A1 (fr) 2001-01-16 2002-09-06 Keymaster Technologies, Inc. Procedes d'identification et de verification
US20030133537A1 (en) 2001-12-05 2003-07-17 Fred Schramm Methods for identification and verification using vacuum XRF system

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See also references of EP2223102A4

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110243810A (zh) * 2019-07-01 2019-09-17 中国第一汽车股份有限公司 一种金属材料表面转化膜中锆含量的测试方法
CN110261198A (zh) * 2019-07-01 2019-09-20 中国第一汽车股份有限公司 一种金属材料表面转化膜中含锆标准测试板的制备方法及其定量方法

Also Published As

Publication number Publication date
AU2015200925B2 (en) 2017-04-06
US20090129541A1 (en) 2009-05-21
WO2009067652A3 (fr) 2009-08-06
EP2223102A2 (fr) 2010-09-01
EP2223102A4 (fr) 2016-09-28
AU2015200925A1 (en) 2015-03-12
AU2008326340A1 (en) 2009-05-28

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